Elias bielouss



nuasnmnouss, or WASHINGTON, ins'rmcr or eonumam,

ASSIGNOR TO HENRY A.

GARDNER, OF WASHINGTON, DISTRICT OF COLUMBIA. PREPARATION OF DRYING OILS.

No Drawing. Application filed July 21, 1920. Serial No. To all whom it may concern:

Be it known that I, ELIAS Bmnouss, a citi- 'zen of the United States, residing at Washington, in the District of Columbia, have invented certain new and useful Improvements in the Preparation of Drying 011s, of

which the following is a specificatlon.

In a co ending application Serial Number 343,458, (fardner and Bielouss, certain methods are described for the preparation of drying oils from chlorinated hydrocarbons, the formation of resinous or asphaltic residues bein largely prevented by a proper. control of't e dechlorinating temperatures, which according to the said apglication are not permitted to exceed 250 for controlling the temperature and otherhydrochloric acid, are apt to while wise facilitating the operation, the said application described the dechlorination of the hydrocarbon in presence of a non-chlorinated diluent, which may be a hydrocarbon or hydrocarbon mixture of the kerosene type. As described in the said application the dech by the addition of certain extraneous substances, such for example as metal owders (iron, zinc, aluminum, etc.),"' or t e like, which function as active catal sts.

My further researches have s own that it is possible, in carrying out the above described processes, to accomplishthe dechlorination without the use of catalysts, and that thereby certain definite advantages are, secured; especially there is, decidedly less liability, even when operating at fairly high temperatures, to the resin-form g condensation; and furthermore somewhat lighter-colored dechlorinated products may be made. appears that catalysts of the type mentioned in the prior application above referred to, in addition to performing their proper function of accelerating the splitting oil of induce certain side reactions which lead eventually to the formation of the objectionable reaction products above referred to as of a resinous character.

at the same time avoiding excessive temperatures, that is to sa temperatures materially exceeding 250 have been able to secure a, practically com lete elimination of the combined chlorin upward of elimination) both with and without the Specification of Letters Iatent.

highly effective solvents for the enamel-lined vessels or As one means lorination is preferably accelerated -This chlorinated. product By omitting the catalyst altogether,

Patented July 12, 1921. 397,872.

use of non-chlorinated diluents, as well as by; the use of'diluents, such as soy oil and bo1led linseed oil, which have a relatively very high boiling point and which, although miscible with the chlorinated and dechlorihated hydrocarbons, are not necessarily resin-like reaction products.

In the practice of the present invention I may effec t the dechlorination in glass or (by operating under anhydrous conditlons) iniron apparatus,

the walls of the latter as are below set forth by way of example. E'wmple I.

A Pennsylvania crude oil, specific gravity 0.741, was topped to 200 C. specific gravity 0.831, was then chlorinated in absence of a catalyst until it had absorbed 52% by weight of chlorin, equivalent to about 34% combined chlorin in the product.

was held at 220- 230 C. for 10 hours in a glass vessel, losin as hydrochloric acid upward of 92% of the combined chlorin. The residual product was a dark colored, rather viscous oil having a specific gravity of 0.961 and an. iodin number of 145. appropriate thinners (mineral spirits, benzene, solvent naphtha, turpentine, etc.) and the addition of 540% of lead-manganese linoleate solution in' turpentine as a drier, the

product yielded highly satisfactory protective films upon metal, .wood, fabrics, etc.,

both with and without pigment additions.

- 1 Example 11.

e residue,

Upon proper dilution by rin. The characteristics of the product were substantially as in Example I, the iodin number in this case being 122.

E (sample I II Mineral spirits, specific gravity 0.815, was chlorinated as bove, yielding a product containing approximately 34.5% of combined chlorinl Upon direct dechlorination at a temperature range of 190 to 205 C., in the absence of any diluent or active catalyst," a dark colored oil resulted of specific gravity 0.938 and an iodin number of 142, this oil on addition of drier, exhibiting satisfactory drying and film-forming qualities.

The dechlorinating operation may be carried out in presence of a non-chlorinated or volatilizable diluent, in which case the operation is preferably conducted under a reflux condenser and approximately at the boilingpoint of the diluent or one of its components, which in the preferred case of mineral spirits is 160220 C. Or it may be carried out at asimilar or somewhat higher tem erature ran e in presence of a high boiling diluent, w ich may be of the glycerid type (soy 'oil, boiled linseed oil, etc.) or, as stated above, the dechlorinating operation may be carried out in absence of any diluent,

.when operating in the formation of resinous products of limited solubility being so far restricted by the proper limitation of the original chlorinating operation, by the proper choice of dechlorinating temperatures, and by the absence of active catalysts, that there is no substantial interference by such resinous products either with the conduct of the operation or with the subsequent recovery and use of the unsaturated oil.

a As regards the limitation of the'chlorinating operation it is my present preference accordance with this invention that the chlorinated product should contain combined chlorin not in excess of about 40% by weight.

I claim 1. A process of preparing drying oils from parafiin-type hydrocarbons, comprising effecting a limited chlorination of the oil, and thereafter dechlorinating the prodnot at moderate temperatures and out of contact with an active catalyst, whereby excessive formation of objectionable by-products of reaction is avoided.

2 Process according to claim lwherein the chlorinated oil contains combined chlorin not in excess of 40% by weight.

In testimony whereof I afiix m signature.

, ELIAS BI LOUSS. 

